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Potassium Carbonate → HCID 13423480, Verbindung

HRID 2164452
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2164452
[NH2:1][C:2]1[O:3][N:4]=[C:5]2[C:10]=1[C:9](=[O:11])[N:8]([CH3:12])[C:7](=[O:13])[N:6]2[CH3:14].[CH2:15](I)[CH2:16][CH3:17].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:12][N:8]1[C:9](=[O:11])[C:10]2=[C:2]([NH:1][CH2:15][CH2:16][CH3:17])[O:3][N:4]=[C:5]2[N:6]([CH3:14])[C:7]1=[O:13]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 126779883-Amino-5,7-dimethyl[1,2]oxazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione

Produkt 1

HCID 13423480HCID 13423480, VerbindungAusbeute 30,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 0.588 g of 3-amino-5,7-dimethyl-isoxazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione, 15 ml of dimethylformamide, 2.5 g of propyl iodide and 1.0 g of potassium carbonate was stirred at 100° C. for 3 hours. From the reaction solution was removed the solvent under reduced pressure. To the residue was added water, which was subjected to extraction with chloroform. The chloroform layer was taken and dried over anhydrous sodium sulfate, from which was removed the solvent. The resultant residue was chromatographed on a column of silica gel (30 g), and the column was eluted with chloroform:acetone:formic acid (20:1:0.1). From the elute was recovered the desired compound, which was recrystallized from isopropyl ether-acetone to give 0.217 g of colorless prisms, melting point: 164°-166° C.

Aufarbeitung

  1. customFrom the reaction solution was removed the solvent under reduced pressure
  2. additionTo the residue was added water, which
  3. extractionwas subjected to extraction with chloroform
  4. dry with materialdried over anhydrous sodium sulfate, from which
  5. customwas removed the solvent
  6. customThe resultant residue was chromatographed on a column of silica gel (30 g)
  7. washthe column was eluted with chloroform:acetone:formic acid (20:1:0.1)
  8. customFrom the elute was recovered the desired compound, which
  9. customwas recrystallized from isopropyl ether-acetone

Quellen und Nachweise

ORD-Eintrag
ord-2a283261039e418397ce59c0010809d2
Quelldatensatz
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04504662

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